反应详情

A solution of phenylethyl magnesium bromide (1M in tetrahydrofuran (40 ml) was added to a stirred solution of 4,5-dihydro 4,4-dimethyl-2-(2,3,4-trimethoxyphenyl) oxazole (5.3 g 0.02M) in dry tetrahydrofuran under a nitrogen atmosphere. The mixture was stirred at 20° for 16 hours. Water (200 ml) was added and the aqueous phase thoroughly extracted with diethyl ether (3×200 ml). The organic solution was dried over magnesium sulphate, filtered and evaporated to leave an oil which was purified by column chromatography on SiO2 eluting with ether/petroleum ether (50/50) to give a colorless oil (6.2 g); MS m/e 339.

1. extractionthe aqueous phase thoroughly extracted with diethyl ether (3×200 ml)
2. dry with materialThe organic solution was dried over magnesium sulphate
3. filtrationfiltered
4. customevaporated
5. customto leave an oil which
6. customwas purified by column chromatography on SiO2 eluting with ether/petroleum ether (50/50)